GB/T 6324.5-2008Test method of organic chemical products -- Part 5: Determination of trace quantities of carbonyl compounds in organic chemicals (English PDF)
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Issued by
General Administration of Quality Supervision, Inspection and Quarantine
Level / Type
National · Recommended
Issue date
June 4, 2008
Implementation date
December 1, 2008
Scope
GB/T 6324.5-2008 (Test method of organic chemical products -- Part 5: Determination of trace quantities of carbonyl compounds in organic chemicals) is available as an English-translated PDF.
GB/T 6324.5-2008 — This Part specifies the test methods for determination of carbonyl compounds in organic chemical products. spectrophotometric method and volumetric method.
This Part is applicable to the determination of carbonyl compounds in water- soluble and alcohol-soluble organic chemical products. The spectrophotometric method is applicable to the sample determination of which carbonyl compound mass fraction is less than or equal to 0.01%.
The volumetric method is applicable to the sample determination of which carbonyl compound mass fraction is greater than 0.01%.
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Document preview — GB/T 6324.5-2008
National Standard of the People's Republic of China
- ICS
- 71.080.01
- Classification
- G 15
Issued by: General Administration of Quality Supervision, Inspection and Quarantine
Contents
- Foreword...3
- 1 Scope...5
- 2 Normative references...5
- 3 Safety and preventative measures...6
- 4 Test method...6
- 5 Expression of results...10
Foreword
GB/T 6324 Test method of organic chemical products consists of six parts.
- Part 1.Water miscibility test of liquid organic chemical products;
- Part 2.Determination of dry residue after evaporation on a water bath for
volatile organic liquids;
- Part 3.Determination of permanganate-reducing substances;
- Part 4.Determination of trace sulfur in organic liquid products -
Microcoulometric method;
- Part 5.Determination of trace quantities of carbonyl compounds in
organic chemicals;
- Part 6.Determination of color for liquids - Tristimulus colorimetry.
This Part is the fifth part of GB/T 6324 and an integrated revision of GB/T
6324.5-1986 and GB/T 6324.6-1986.
The revision of this Part adopts the Standard of American Society for Testing
and Materials ASTM E 411-2005 Standard Test Method for Trace Quantities of
Carbonyl Compounds with 2,4-Dinitrophenylhydrazine (English version).
This Part was redrafted based on ASTM E 411-2005.Annex A lists the
comparison on clause number between this Part and ASTM E 411-2005.
Considering national conditions of China, this Part made some modifications
when adopting ASTM E 411-2005.The main difference is as follows.
- added determination of carbonyl compounds - volumetric method (4.2 of
this Part), so as to cooperate with the change of the method
determination range.
This Part replaces GB/T 6324.5-1986 Organic chemical products for industrial
use--Determination of content of carbonyl compounds present--Volumetric
method and GB/T 6324.6-1986 Organic chemical products for industrial use--
Determination of content of carbonyl compounds present in small amounts--
Photometric method.
Compared with GB/T 6324.5-1986 and GB/T 6324.6-1986, the main changes
are as follows.
- modified the name of this Part from "Organic chemical products for
industrial use--Determination of content of carbonyl compounds present"
to "Test method of organic chemical products - Part 5.Determination of
trace quantities of carbonyl compounds in organic chemicals" (cover of
Edition 1986, cover of this Edition);
- made the corresponding changes for "Scope" (Clause 1 of Edition 1986,
Clause 1 of this Edition);
- added spectrophotometric method (see 4.2);
- in the spectrophotometric method, it modified the standard substance
from acetophenone to 2-butanone, test temperature from 50°C to room
temperature, color development time from 5 min to 12 min, color
development wavelength from 445 nm to 480 nm; modified "use ethanol
to adjust the instrument zero point " to "adjust the zero point of the
spectrophotometer with water" (3.5 and Clause 5 of Edition 1986, 4.2.2.5
and 4.2.4 of this Edition);
- in volumetric method, it added that when the endpoint color change is not
obvious, it could use the potentiometric method to determine the end (see
4.3).
Annex A of this Part is informative.
This Part was proposed by China Petroleum and Chemical Industry Association.
This Part shall be under the jurisdiction of Subcommittee on Organic, National
Technical Committee on Chemical of Standardization Administration of China
(SAC/TC 63 / SC 2).
Main drafting organizations of this Part. Jinan IFT Science & Technology Co.,
Ltd., Shandong Chemical Research Institute.
The drafting organization of this Part. China Petrochemical Corporation Jinzhou
Petrochemical Company.
Main drafter of this Part. Qiu Juan, Cui Aihong, Yu Pengling, Qi Xinyu, Li Debo.
Versions of standard substituted by this Standard are.
- GB/T 6324.5-1986, GB/T 6324.6-1986.
Test method of organic chemical products –
Part 5.Determination of trace quantities of carbonyl
compounds in organic chemicals
WARNING This Part does not address all safety issues related to the use
of standards. It is user's responsibility to take appropriate safety and
protective measures and to ensure compliance with the relevant national
regulations. See Clause 3 for information on safety and precautionary
measures.
1 Scope
This Part specifies the test methods for determination of carbonyl compounds
in organic chemical products. spectrophotometric method and volumetric
method.
This Part is applicable to the determination of carbonyl compounds in water-
soluble and alcohol-soluble organic chemical products. The spectrophotometric
method is applicable to the sample determination of which carbonyl compound
mass fraction is less than or equal to 0.01%. The volumetric method is
applicable to the sample determination of which carbonyl compound mass
fraction is greater than 0.01%.
2 Normative references
The following standards contain the provisions which, through reference in this
Part, constitute the provisions of this Part. For dated references, subsequent
amendments (excluding corrections) or revisions do not apply to this Part.
However, the parties who enter into agreement based on this Part are
encouraged to investigate whether the latest versions of these documents are
applicable. For undated reference documents, the latest versions apply to this
Part.
GB/T 601-2002 Chemical Reagent - Preparations of Standard Volumetric
Solutions
GB/T 603-2002 Chemical Reagent - Preparations of Reagent Solution for
Use in Test (ISO 6353-1.1982, NEQ)
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods (eqv ISO 3696.1987)
3 Safety and preventative measures
3.1 Sampling safety shall be specified in the product standard according to
product characteristics.
3.2 Methanol is flammable. It may be on fire in distillation. So it should take
preventive measures. For example, inspect the flask for cracks;
3.3 2,4-dinitrophenylhydrazine is easy to explode. Open flame or electric
spark can make it intense burning. Avoid heat sources during use.
4 Test method
4.1 General
Unless otherwise stated, only reagents identified as analytically pure and grade
3 water as specified in GB/T 6682-2008 can be used in the analysis.
4.2 Spectrophotometric method
4.2.1 Methodology
The carbonyl compounds in the sample react with 2,4-dinitrophenylhydrazine
in acidic medium to generate 2,4-dinitrophenylhydrazone. 2,4-
dinitrophenylhydrazone reacts with potassium hydroxide, resulting in significant
red material. Measure the absorbance with a spectrophotometer at a
wavelength of 480 nm to obtain carbonyl compound content.
Equation.
4.2.2 Reagents and solutions
4.2.2.4 2,4-dinitrophenylhydrazine solution. 1 g/L
4.2.2.5 Carbonyl compound standard solution (in CO). 2.5 mg/mL
Weigh 0.643 g of 2-butanone dissolved in about 50 mL of carbonyl-free
methanol. Transfer it to a 100 mL volumetric flask. Use carbonyl-free methanol
to dilute it to the scale. Shake it well.
4.2.3 Apparatus
Spectrophotometer. with a cuvette of which the optical path is 1 cm; absorbance
accuracy is ± 0.004 (A).
4.2.4 Analysis procedure
4.2.4.1 Standard curve drawing
4.2.4.2 Sample determination
4.2.4.2.1 Preparation of sample solution
Pipet 2.0 mL of laboratory sample containing (0.5 ~ 50) µg of carbonyl in a pre-
weighed 25 mL volumetric flask. Weigh it to the nearest of 0.0001 g. The
difference between the two weighings shall be the mass of the laboratory
sample.
4.2.5 Calculation of results
The mass fraction w1 of carbonyl compound, in carbonyl (CO), values in %,
shall be calculated according to equation (1).
4.3 Volumetric method
4.3.1 Methodology
The carbonyl compound in the sample is reacted with hydroxylamine
hydrochloride. The resulting acid shall be indicated in bromophenol blue. Use
sodium hydroxide standard titration solution to titrate. Calculate the content of
carbonyl compound.
4.3.2 Reagents and solutions
4.3.2.1 95% ethanol
4.3.3 Apparatus
Micro-burette. 10 mL
4.3.4 Analysis procedures
Weigh 50 mL of hydrochloric acid hydroxylamine solution and place it in a 250
mL iodometric flask used as standard color for titration.
5 Expression of results
Take the arithmetic mean of the results of two parallel determinations as the
measurement result.
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 10 pages — is available in the English PDF.
Referenced standards
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Related Standards
GB/T 6682-2008 — Water for analytical laboratory use - Specification and test methods
GB/T 6324.1-2004 — Test method of organic chemical products -- Part 1: Water miscibility test of liquid organic chemical products
GB/T 6324.10-2020 — Test method of organic chemical products - Part 10: Determination of trace sulfur in organic liquid products - Ultraviolet fluorescence method
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